High resolution capillary gas chromatography and gas chromatography-mass spectrometry of protein and non-protein amino acids, amino alcohols, and hydroxycarboxylic acids as theirtert-butyldimethylsilyl derivatives

✍ Scribed by Šimek, Petr ;Heydová, Anna ;Jegorov, Alexandr

• Publisher: John Wiley and Sons
• Year: 1994
• Tongue: English
• Weight: 784 KB
• Volume: 17
• Category: Article
• ISSN: 0935-6304
• DOI: 10.1002/jhrc.1240170305

✦ Synopsis

Abstract

A simple, single‐step derivatization technique is presented for capillary GC‐FID and GC‐MS separation and identification of common protein and non‐protein constituents of natural peptides as their tert‐butyldimethylsilyl (TBDMS) derivatives. The tert‐butyldimethyl‐silylation of more than sixty compounds was accomplished with high yields and a single peak observed for each component. The TBDMS derivatives of both the protein and non‐protein substances, moreover, exhibit excellent separation on apolar capillary columns and can be resolved completely using a polydimethylsiloxane or 5 % phenyl polydimethylsiloxane column and, complementarily, a 50 % phenyl polydimethylsiloxane column. Retention data and molar responses of the TBDMS derivatives on the polydimethylsiloxane column are compiled. Direct coupling of the 5 % phenyl polydimethylsiloxane column to an ion trap mass spectrometer enabled fast separation and identification of the investigated components, at nanomole to picomole levels, on the basis of retention and mass spectral data. The general usefulness of the method is demonstrated by research into new biologically active peptides isolated from entomopathogenic fungi.